2-Aminopyrimidine → HCID 20544711, 화합물

HRID 2285506노트

반응식

HRID 2285506 반응식
[NH2:1][C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[Cl:8][C:9]1[CH:18]=[CH:17][C:12]2[O:13][CH2:14][CH2:15][O:16][C:11]=2[C:10]=1[C:19](Cl)=[O:20]>C(C(C)=O)C>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[NH:1][C:19]([C:10]1[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=2[CH:17]=[CH:18][C:9]=1[Cl:8])=[O:20]

참가 물질

4

반응물 2

HCID 79782-AminopyrimidineHCID 20544693HCID 20544693, 화합물

생성물 1

HCID 20544711HCID 20544711, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
10 °C

실험 절차

280 ml of methyl ethyl ketone, 13 g of 2-amino-pyrimidine were put into a 500 ml balloon flask provided with a stirrer and a thermometer. The mixture was cooled to 10° C. and 28 g of ground 6-chloro-1,4-benzodioxane-5-carbonyl chloride was added and stirred for two hours, the temperature being allowed to rise to 20° C. The obtained solid was filtered off, washed with 30 ml of methyl ethyl ketone and then dissolved in 250 ml of boiling water. The solution was treated with 10 ml of 36° Bel caustic soda lye. After filtration 12 g of product were obtained and crystallized again from 150 ml of ethanol. 9.5 g of N-(2-pyrimidyl)-6-chloro-1,4-benzodioxane-5-carboxamide was obtained. (M.P.: 223° C. with decomposition). The structure was confirmed by nuclear magnetic resonance analysis.

후처리

  1. customprovided with a stirrer
  2. customto rise to 20° C
  3. filtrationThe obtained solid was filtered off
  4. washwashed with 30 ml of methyl ethyl ketone
  5. dissolutiondissolved in 250 ml of boiling water
  6. additionThe solution was treated with 10 ml of 36° Bel caustic soda lye
  7. filtrationAfter filtration 12 g of product
  8. customwere obtained
  9. customcrystallized again from 150 ml of ethanol

출처 및 근거

ORD 기록
ord-7d008ccd6a46465d99976d0215927d8b
출처 데이터셋
uspto-grants-1982_04
특허 번호
US04323503

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